ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Trifluoroacetic acid → N-(2-((6-(3-(2,6-dichloro-3,5-dimethoxyphenyl)-1-methylureido)pyrimidin-4-yl)amino)-5-(piperazin-1-yl)phenyl)acrylamide

HRID 58205
ノート
印刷プレビュー

反応式

HRID 58205 の反応式
[C:1]([NH:5][C:6]1[CH:7]=[C:8]([N:51]2[CH2:56][CH2:55][N:54](C(OC(C)(C)C)=O)[CH2:53][CH2:52]2)[CH:9]=[CH:10][C:11]=1[N:12](C(OC(C)(C)C)=O)[C:13]1[CH:18]=[C:17]([N:19]([CH3:43])[C:20]([N:22]([C:31]2[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[CH:34]=[C:33]([O:40][CH3:41])[C:32]=2[Cl:42])COCC[Si](C)(C)C)=[O:21])[N:16]=[CH:15][N:14]=1)(=[O:4])[CH:2]=[CH2:3].C(O)(C(F)(F)F)=O.[NH4+].[OH-]>C(Cl)Cl>[Cl:37][C:36]1[C:35]([O:38][CH3:39])=[CH:34][C:33]([O:40][CH3:41])=[C:32]([Cl:42])[C:31]=1[NH:22][C:20](=[O:21])[N:19]([C:17]1[N:16]=[CH:15][N:14]=[C:13]([NH:12][C:11]2[CH:10]=[CH:9][C:8]([N:51]3[CH2:52][CH2:53][NH:54][CH2:55][CH2:56]3)=[CH:7][C:6]=2[NH:5][C:1](=[O:4])[CH:2]=[CH2:3])[CH:18]=1)[CH3:43]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 14923Ammonium HydroxideHCID 131736987HCID 131736987、化合物

生成物 1

HCID 118025964N-(2-((6-(3-(2,6-dichloro-3,5-dimethoxyphenyl)-1-methylureido)pyrimidin-4-yl)amino)-5-(piperazin-1-yl)phenyl)acrylamide収率 94.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

tert-butyl 4-(3-acrylamido-4-((tert-butoxycarbonyl)(6-(3-(2,6-dichloro-3,5-dimethoxyphenyl)-1-methyl-3-((2-(trimethylsilyl)ethoxy)methyl)ureido)pyrimidin-4-yl)amino)phenyl)piperazine-1-carboxylate (59 g, 0.06 mmol) was stirred in DCM (2.0 ml). TFA (97 μl, 1.3 mmol) was added and the mixture was stirred at room temperature for 6 hours. The reaction mixture was evaporated. The remaining residue was dissolved in DCM and washed with saturated NaHCO3, dried over MgSO4 and evaporated. The resulting material was dissolved in THF (2.0 ml) and NH4OH (74 μl, 1.9 mmol) was added. The reaction mixture was stirred at room temperature for 5 minutes. The reaction mixture was evaporated to obtain the title compound (34 mg, yield: 90%) which was taken to the next step without further purification. 1H-NMR (400 MHz, DMSO-d) δ 2.62 (br. s., 4H) 3.08-3.27 (m, 7H) 3.77-4.03 (m, 6H) 5.72 (d, 1H) 6.11-6.34 (m, 2H) 6.40-6.62 (m, 1H) 6.70-6.98 (m, 2H) 7.22-7.37 (m, 2H) 8.32 (s, 1H) 8.70 (s, 1H) 9.58 (br. s., 1H) 12.06 (s, 1H); ESI-MS: 601 [M+H]+.

後処理

  1. customThe reaction mixture was evaporated
  2. dissolutionThe remaining residue was dissolved in DCM
  3. washwashed with saturated NaHCO3
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. dissolutionThe resulting material was dissolved in THF (2.0 ml)
  7. stirringThe reaction mixture was stirred at room temperature for 5 minutes
  8. customThe reaction mixture was evaporated

出典と根拠

ORDレコード
ord-2befc5d1073041cb9ce92f229076431d
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434697B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート